CN1449806A - Technology for producing Liuwei Dihuang Wan - Google Patents

Technology for producing Liuwei Dihuang Wan Download PDF

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Publication number
CN1449806A
CN1449806A CN 03117152 CN03117152A CN1449806A CN 1449806 A CN1449806 A CN 1449806A CN 03117152 CN03117152 CN 03117152 CN 03117152 A CN03117152 A CN 03117152A CN 1449806 A CN1449806 A CN 1449806A
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China
Prior art keywords
thick paste
extract
cortex moutan
fructus corni
filtrate
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CN 03117152
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Chinese (zh)
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康国忠
赵汉臣
陈萍
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Individual
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Individual
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Priority to CN 03117152 priority Critical patent/CN1449806A/en
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Abstract

The production process of Chinese medicine six-ingredient rehmannia pill includes the following steps: using CO2 supercritical fluid to respectively extract the Chinese medicinal materials of moutan root bark and alisma tuber; decocting other medicinal materials to obtain decoction, filtering the decoction to obtain the filtrate; adopting ultrafiltration membrane with different specification to make gradient filtration and separation so as to obtain the invention product six-ingredient rehmannia pill. As compared with existent technology said invented production process can completely remain their polysaccharide component with important medicine effect, and can raise yield.

Description

The production technology of Chinese medicine Liuwei Dihuang preparation
Technical field: the present invention is a kind of production technology of Chinese medicine Liuwei Dihuang preparation, belongs to medicine, the particularly production technology of Chinese medicine medicine.
Technical background: the applicant soars comrade and once submitted to a number of patent application to be to Patent Office of the People's Republic of China: 02134148.6, name is called the patent application of " production technology of LIUWEIDIHUANG JIAONANG ", we find to exist certain problem in actual production process and medicine use thereof: mainly be still to have certain impurity and invalid element in the medicine, drug quality stability is not strong, recovery rate is low in the production process, simultaneously utilize decocting to boil fully and the method for alcohol extraction, because temperatures involved, can produce destruction to active ingredient in the medicine, the polysaccharide component that has important drug action in the medicine can not separate by different molecular weight, so it is kept fully, the polysaccharide composition incurs loss in the macroporous resin adsorption separation process, some macromole invalid elements of while, as: starch, phlegmatic temperaments etc. still are retained in the medicine, increase the dose of patient to this medicine, and energy consumption is bigger in the production process, the cost height, environment there is certain pollution, quality is difficult for controlled, does not meet the production requirement of the modernization of Chinese medicine.
Summary of the invention: the objective of the invention is to: the production technology that a kind of Chinese medicine Liuwei Dihuang preparation is provided, it be utilize the method for CO2 supercritical fluid extraction in the prior art and utilize membrane separation technique to finish of the present invention, so, improved recovery rate, avoided the destruction of high temperature active ingredient, simultaneously reached the purpose that cuts down the consumption of energy again, reduced pollution environment; The polysaccharide component that has important drug action in the medicine separates by different molecular weight, it is kept fully, avoid the polysaccharide composition in the separation process of prior art macroporous resin adsorption, to lose, removed simultaneously the macromole invalid element fully, can directly carry out cold drying and separate the polysaccharide that obtains for the thick paste shape, do not need to concentrate again, reach purpose of energy saving; The present invention is achieved in that Six-element Chinese medicine preparation being defined as according to state-promulgated pharmacopoeia: Radix Rehmanniae Preparata, Fructus Corni, Cortex Moutan, Rhizoma Dioscoreae, Poria, Rhizoma Alismatis, the material Cortex Moutan of getting it filled, Rhizoma Alismatis extracts with the CO2 supercritical fluid respectively, the extract and the medicinal residues that obtain are standby, get Fructus Corni and add alcohol reflux, filter, medicinal residues are standby, filtrate recycling ethanol, be concentrated into thick paste, get above-mentioned Cortex Moutan, Rhizoma Alismatis, Fructus Corni medicinal residues and Radix Rehmanniae Preparata, Rhizoma Dioscoreae, Poria decocts with water, filter, merging filtrate, get filtrate and carry out the gradient isolated by filtration with the ultrafilter membrane of different size, liquid on the thick paste shape film
Liquid passes through macroporous resin column under the above-mentioned film, ethanol gradient elution is collected eluent, reclaims ethanol, be concentrated into the thick paste shape, add above-mentioned Rhizoma Alismatis extract, Fructus Corni alcohol extraction thick paste, membrane filtration thick paste, mixing, drying under reduced pressure, be ground into fine powder, add Cortex Moutan extract and appropriate amount of auxiliary materials again, mixing makes the Chinese medicine Liuwei Dihuang preparation; Method particularly is: material Cortex Moutan 528 grams of getting it filled, Rhizoma Alismatis 538 grams extract with the CO2 supercritical fluid respectively, and extract and medicinal residues are standby; Get Fructus Corni 704 grams and add alcohol reflux, filter, medicinal residues are standby, and filtrate recycling ethanol is concentrated into thick paste; Get above-mentioned Cortex Moutan, Rhizoma Alismatis, Fructus Corni medicinal residues and Radix Rehmanniae Preparata 1408 grams, Rhizoma Dioscoreae 704 grams, Poria 528 grams decoct with water, filter, merging filtrate, get filtrate and carry out the gradient isolated by filtration with the ultrafilter membrane of the sub-very much magnitude of 5-10, discard liquid on the film, the ultrafilter membrane of the sub-very much magnitude of filtrate reuse 0.1-0.3 carries out the gradient isolated by filtration, get liquid on the thick paste shape film, liquid passes through macroporous resin column under the film, ethanol gradient elution, collect eluent, reclaim ethanol, be concentrated into the thick paste shape, add above-mentioned Rhizoma Alismatis extract, Fructus Corni alcohol extraction thick paste, the membrane filtration thick paste, mixing, drying under reduced pressure is ground into fine powder, adds Cortex Moutan extract and appropriate amount of auxiliary materials, mixing is made the preparation of different dosage form; Preparation of the present invention is any oral dosage form, comprising: capsule, granule, tablet, pill, drop pill, oral liquid, DIXIN SHUIWAN.Compared with prior art: the present invention has and utilizes the advantage that the CO2 supercritical fluid extraction is pollution-free, post processing is easy, the steam distillation that replacing prior art provides extracts volatile component and fat-soluble composition, improved recovery rate, recovery rate of the present invention is 2~3 times of steam distillation, avoided the destruction of high temperature again to active ingredient, simultaneously reached the purpose that cuts down the consumption of energy again, reduced pollution environment; Utilize membrane separation technique to carry out before the macroporous resin adsorption separation polysaccharide composition with important drug action being separated by different molecular weight at water cooking liquid, it is kept fully, avoid the polysaccharide composition in the separation process of prior art macroporous resin adsorption, to lose, removed simultaneously the macromole invalid element fully, as: starch, phlegmatic temperaments etc. are because the medicine active ingredient refine more of preparation, so under square one, can reduce the amount that the patient takes medicine again, alleviate patient's mental burden; Can directly carry out cold drying and separate the polysaccharide that obtains for the thick paste shape, do not need to concentrate again, reach purpose of energy saving, though the present invention has increased certain operation, improved the scientific and technological content of product, extract active component to greatest extent and remove invalid element fully, reduced heating process significantly, reduce the destruction of high temperature, meet more or, reached the purpose of invention near the requirement of the modernization of Chinese medicine to active ingredient.
Embodiments of the invention 1: material Cortex Moutan 528 grams of getting it filled, Rhizoma Alismatis 538 grams extract with the CO2 supercritical fluid respectively, and extract and medicinal residues are standby; Get Fructus Corni 704 grams and add alcohol reflux, filter, medicinal residues are standby, and filtrate recycling ethanol is concentrated into thick paste; Get above-mentioned Cortex Moutan, Rhizoma Alismatis, Fructus Corni medicinal residues and Radix Rehmanniae Preparata 1408 grams, Rhizoma Dioscoreae 704 grams, Poria 528 grams decoct with water, filter, merging filtrate, get filtrate and carry out the gradient isolated by filtration with the ultrafilter membrane of the sub-very much magnitude of 5-10, discard liquid on the film, the ultrafilter membrane of the sub-very much magnitude of filtrate reuse 0.1-0.3 carries out the gradient isolated by filtration, get liquid on the thick paste shape film, liquid passes through macroporous resin column under the film, ethanol gradient elution, collect eluent, reclaim ethanol, be concentrated into the thick paste shape, add above-mentioned Rhizoma Alismatis extract, Fructus Corni alcohol extraction thick paste, the membrane filtration thick paste, mixing, drying under reduced pressure is ground into fine powder, adds Cortex Moutan extract and appropriate amount of auxiliary materials, in incapsulating behind the mixing, get 1000 granule products.
Embodiments of the invention 2: according to the ratio of pharmacopeia regulation, the material Cortex Moutan of getting it filled, Rhizoma Alismatis extracts with the CO2 supercritical fluid respectively, the extract and the medicinal residues that obtain are standby, get Fructus Corni and add alcohol reflux, filter, medicinal residues are standby, filtrate recycling ethanol, be concentrated into thick paste, get above-mentioned Cortex Moutan, Rhizoma Alismatis, Fructus Corni medicinal residues and Radix Rehmanniae Preparata, Rhizoma Dioscoreae, Poria decocts with water, filter, merging filtrate, get filtrate with 50,000,70,000, the ultrafilter membrane of 10 sub-very much magnitudes carries out isolated by filtration respectively, all discard liquid on the film, filtrate reuse 0.1 ten thousand, 0.2 ten thousand, 0.3 the ultrafilter membrane of sub-very much magnitude carries out isolated by filtration, get liquid on the thick paste shape film, liquid passes through macroporous resin column according to prior art under the above-mentioned film, ethanol gradient elution, collect eluent, reclaim ethanol, be concentrated into the thick paste shape, add the Rhizoma Alismatis extract that has obtained, Fructus Corni alcohol extraction thick paste, the membrane filtration thick paste, mixing, drying under reduced pressure, be ground into fine powder, add Cortex Moutan extract and appropriate amount of auxiliary materials again, mixing makes Chinese medicine six drugs containing rehmanniae tablet according to conventional method.
Embodiments of the invention 3: according to the ratio of pharmacopeia regulation, the material Cortex Moutan of getting it filled, Rhizoma Alismatis extracts with the CO2 supercritical fluid respectively, the extract and the medicinal residues that obtain are standby, get Fructus Corni and add alcohol reflux, filter, medicinal residues are standby, filtrate recycling ethanol is concentrated into thick paste, gets above-mentioned Cortex Moutan, Rhizoma Alismatis, Fructus Corni medicinal residues and Radix Rehmanniae Preparata, Rhizoma Dioscoreae, Poria decocts with water, filter, merging filtrate, get filtrate and carry out isolated by filtration with the ultrafilter membrane of 5 sub-very much magnitudes, all discard liquid on the film, the ultrafilter membrane of the sub-very much magnitude of filtrate reuse 0.3 carries out isolated by filtration, gets liquid on the thick paste shape film, liquid passes through macroporous resin column under the above-mentioned film, ethanol gradient elution is collected eluent, reclaims ethanol, be concentrated into the thick paste shape, add above-mentioned Rhizoma Alismatis extract, Fructus Corni alcohol extraction thick paste, the membrane filtration thick paste, mixing, drying under reduced pressure, be ground into fine powder, add Cortex Moutan extract and appropriate amount of auxiliary materials again, mixing is produced Chinese medicine six drugs containing rehmanniae sustained-release particle formulation according to conventional method.
Embodiments of the invention 4: according to the ratio of pharmacopeia regulation, the material Cortex Moutan of getting it filled, Rhizoma Alismatis extracts with the CO2 supercritical fluid respectively, the extract and the medicinal residues that obtain are standby, get Fructus Corni and add alcohol reflux, filter, medicinal residues are standby, filtrate recycling ethanol is concentrated into thick paste, gets above-mentioned Cortex Moutan, Rhizoma Alismatis, Fructus Corni medicinal residues and Radix Rehmanniae Preparata, Rhizoma Dioscoreae, Poria decocts with water, filter, merging filtrate, get filtrate and carry out isolated by filtration with the ultrafilter membrane of 10 sub-very much magnitudes, all discard liquid on the film, the ultrafilter membrane of the sub-very much magnitude of filtrate reuse 0.1 carries out isolated by filtration, gets liquid on the thick paste shape film, liquid passes through macroporous resin column under the above-mentioned film, ethanol gradient elution is collected eluent, reclaims ethanol, be concentrated into the thick paste shape, add above-mentioned Rhizoma Alismatis extract, Fructus Corni alcohol extraction thick paste, the membrane filtration thick paste, mixing, drying under reduced pressure, be ground into fine powder, add Cortex Moutan extract and appropriate amount of auxiliary materials again, mixing is produced Chinese medicine six drugs containing rehmanniae oral liquid formulations according to conventional method.

Claims (3)

1, a kind of production technology of Chinese medicine Liuwei Dihuang preparation, Six-element Chinese medicine preparation wherein is: Radix Rehmanniae Preparata, Fructus Corni, Cortex Moutan, Rhizoma Dioscoreae, Poria, Rhizoma Alismatis, it is characterized in that: the material Cortex Moutan of getting it filled, Rhizoma Alismatis extracts with the CO2 supercritical fluid respectively, the extract and the medicinal residues that obtain are standby, get Fructus Corni and add alcohol reflux, filter, medicinal residues are standby, filtrate recycling ethanol, be concentrated into thick paste, get above-mentioned Cortex Moutan, Rhizoma Alismatis, Fructus Corni medicinal residues and Radix Rehmanniae Preparata, Rhizoma Dioscoreae, Poria decocts with water, filter, merging filtrate is got filtrate and is carried out the gradient isolated by filtration with the ultrafilter membrane of different size, liquid on the thick paste shape film, liquid passes through macroporous resin column under the above-mentioned film, ethanol gradient elution is collected eluent, reclaims ethanol, be concentrated into the thick paste shape, add above-mentioned Rhizoma Alismatis extract, Fructus Corni alcohol extraction thick paste, the membrane filtration thick paste, mixing, drying under reduced pressure, be ground into fine powder, add Cortex Moutan extract and appropriate amount of auxiliary materials again, mixing makes the Chinese medicine Liuwei Dihuang preparation.
2, according to the production technology of the described Chinese medicine Liuwei Dihuang preparation of claim 1, it is characterized in that: material Cortex Moutan 528 grams of getting it filled, Rhizoma Alismatis 538 grams extract with the CO2 supercritical fluid respectively, and extract and medicinal residues are standby; Get Fructus Corni 704 grams and add alcohol reflux, filter, medicinal residues are standby, and filtrate recycling ethanol is concentrated into thick paste; Get above-mentioned Cortex Moutan, Rhizoma Alismatis, Fructus Corni medicinal residues and Radix Rehmanniae Preparata 1408 grams, Rhizoma Dioscoreae 704 grams, Poria 528 grams decoct with water, filter, merging filtrate, get filtrate and carry out the gradient isolated by filtration with the ultrafilter membrane of the sub-very much magnitude of 5-10, discard liquid on the film, the ultrafilter membrane of the sub-very much magnitude of filtrate reuse 0.1-0.3 carries out the gradient isolated by filtration, get liquid on the thick paste shape film, liquid passes through macroporous resin column under the film, ethanol gradient elution, collect eluent, reclaim ethanol, be concentrated into the thick paste shape, add above-mentioned Rhizoma Alismatis extract, Fructus Corni alcohol extraction thick paste, the membrane filtration thick paste, mixing, drying under reduced pressure is ground into fine powder, adds Cortex Moutan extract and appropriate amount of auxiliary materials, mixing is made the preparation of different dosage form.
3, according to the production technology of claim 1,2 described Chinese medicine Liuwei Dihuang preparations, it is characterized in that: described preparation is any oral dosage form, comprising: capsule, granule, tablet, pill, drop pill, oral liquid, DIXIN SHUIWAN.
CN 03117152 2003-01-10 2003-01-10 Technology for producing Liuwei Dihuang Wan Pending CN1449806A (en)

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN100344309C (en) * 2005-03-15 2007-10-24 江中药业股份有限公司 Refining method for Liuweidihuang compound preparation by membrane technology separation
CN100500193C (en) * 2003-08-19 2009-06-17 中国人民解放军军事医学科学院毒物药物研究所 Extract from decoction of rehmannia including six elements, combination of medication, and medical use
CN101167923B (en) * 2007-10-31 2010-10-27 兰州卷烟厂 Preparation of six ingredients with rehmannia and its application in cigarette
CN101167924B (en) * 2007-11-02 2010-12-01 湖南大学 Method for producing traditional Chinese medicine preparation of six ingredients with rehmannia
CN104887905A (en) * 2015-06-26 2015-09-09 赵明亮 Preparation method for six-ingredient rehmannia pills and application thereof

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN100500193C (en) * 2003-08-19 2009-06-17 中国人民解放军军事医学科学院毒物药物研究所 Extract from decoction of rehmannia including six elements, combination of medication, and medical use
CN100344309C (en) * 2005-03-15 2007-10-24 江中药业股份有限公司 Refining method for Liuweidihuang compound preparation by membrane technology separation
CN101167923B (en) * 2007-10-31 2010-10-27 兰州卷烟厂 Preparation of six ingredients with rehmannia and its application in cigarette
CN101167924B (en) * 2007-11-02 2010-12-01 湖南大学 Method for producing traditional Chinese medicine preparation of six ingredients with rehmannia
CN104887905A (en) * 2015-06-26 2015-09-09 赵明亮 Preparation method for six-ingredient rehmannia pills and application thereof

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